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The synthesis and the X-ray structure of the Zn(II) zwitterionic complex:1-ethylpiperaziniumtrichlorozincate (II) are described. In the atomic arrangement, the ZnCl 3 N entities, grouped in pairs, are deployed along the b -axis to form layers. The organic entities are inserted between these layers through N H⋯Cl and C H⋯Cl hydrogen bonds to form infinite three-dimensional network. The 3D Hirshfeld surfaces were investigated for intermolecular interactions. The optimized geometry, Mulliken charge distribution, molecular electrostatic potential (MEP) maps and thermodynamic properties have been calculated using the Lee-Yang-Parr correlation functional B3LYP with the LanL2DZ basis set. The HOMO and LUMO energy gap and chemical reactivity parameters were made. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray crystal structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and of the IR bands. [ABSTRACT FROM AUTHOR]

The crystal structure of the new complex [Co(C 5 H 7 N 3 O) 2 (H 2 O) 4 ](NO 3 ) 2 ⋅4H 2 O synthesized in aqueous solution has been determined by single crystal X-ray diffraction. The compound crystallizes in the triclinic space group P 1 ¯ with lattice parameters: a = 7.3056(2), b = 8.4065(2), c = 10.4724(3) Å, α = 103.9470(19), β = 105.6600(14), γ = 91.1350(18)°, V = 598.54(3) Å 3 and Z = 1. The Co(II) central ion is in a slightly distorted octahedral coordination geometry formed by two nitrogen atoms of two 2-amino-6-methoxypyrimidine ligands and four oxygen atoms of coordinated water molecules. The crystal packing is stabilized by intermolecular O H⋯O, N H⋯O and C H⋯O hydrogen bonds which link the molecules into a three-dimensional network. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived. The vibrational absorption bands were identified by infrared spectroscopy. The compound was characterized by thermal analysis to determine its thermal behavior with respect to temperature. [ABSTRACT FROM AUTHOR]

The Zn(II) complex with the monodentate ligand 4-fluoroaniline, ZnCl 2 (C 6 H 4 FNH 2 ) 2 , has been prepared and characterized by single crystal X-ray diffraction, solid state nuclear magnetic resonance, infrared spectroscopy and differential scanning calorimetry. The Zn(II) ion is tetracoordinated by two nitrogen atoms of two monodentate 4-fluoroaniline ligands and two chlorine atoms. In the molecular arrangement, the ZnCl 2 (C 6 H 4 FNH 2 ) 2 entities are interconnected via N H⋯Cl hydrogen bonds to form layers parallel to the ( a , b ) plane. The nature and proportion of contacts in the crystal packing were investigated through the Hirshfeld surfaces. The crystal is mainly maintained by electrostatic attractions Cl − … H N and by extensive hydrophobic contacts as revealed by the Hirshfeld 2D fingerprint plots and statistical analysis. The 13 C and 19 F CP-MAS NMR spectra are in agreement with the X-ray structure and confirm the phase purity of the crystalline sample. The vibrational absorption bands were identified by infrared spectroscopy. A calorimetric study shows that the title compound is stable until 262.5 °C. [ABSTRACT FROM AUTHOR]

The synthesis, crystal structure and spectroscopic characterization of a new chlorocadmate template by the 1-(2-hydroxyethyl)piperazine ligand are reported. In the atomic arrangement, the CdCl 5 O entities are deployed in corrugated rows along the a -axis at y = 1/4 and y = 3/4 to form layers parallel to the ( a,b ) plane. In these crystals, piperazinediium cations are in a chair conformation and are inserted between these layers through N H⋯Cl, C H⋯Cl, O H⋯Cl and N H⋯O hydrogen bonds to form infinite three-dimensional network. Investigation of intermolecular interactions and crystal packing via Hirshfeld surface analysis reveals that H⋯Cl and C H⋯H C intermolecular interactions are the most abundant contacts of the organic cation in the crystal packing. The crystal contacts enrichments reveals that, the Cd ++ … Cl − salt bridges, the Cd⋯O complexation and O H⋯Cl- and N H⋯Cl-strong H-bonds are the driving forces in the packing formation. The presence of twelve independent chloride anions and four organic cation in the asymmetric unit allowed comparing their contact propensities. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. Additional characterization of this compound has also been performed by IR spectroscopy. [ABSTRACT FROM AUTHOR]

The synthesis, crystal structure and spectroscopic characterization of the novel 1-(2-hydroxyethyl)piperaziniumtrichlorozincate(II) zwitterionic complex are reported. In the atomic arrangement, the ZnCl 3 N entities, grouped in pairs, are deployed in rows along the a -axis to form layers parallel to the ( a , c ) plane. The organic molecules are inserted between these layers through N-H…Cl, C-H…Cl, O-H…Cl and N-H…O hydrogen bonds to form infinite three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and of the IR bands. [ABSTRACT FROM AUTHOR]

1-Ethylpiperazinediium pentachloroantimonate (III) monohydrate, C 6 H 16 N 2 SbCl 5 ·H 2 O, has been synthesized by the reaction of antimony trioxide (Sb 2 O 3 ) and 1-ethylpiperazine in an aqueous solution of hydrochloric acid. The structure crystallizes in orthorhombic system, in the non-centrosymmetric space group Pca 2 1 and consists of isolated [C 6 H 16 N 2 ] 2+ cations, square pyramidal [SbCl 5 ] 2− anions and lattice water molecules. O H⋯Cl hydrogen bonds link the [SbCl 5 ] 2− anions and water molecules to form double chains stretching along the [101] direction. The chains in turn are linked to the organic cations via N H⋯Cl, C H⋯Cl, C H⋯O and N H⋯O hydrogen bonds to form a three-dimensional network. This structure presents an example of a general square pyramidal complex ion containing a stereo-chemically active lone pair of electrons. Solid state 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure, and vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and IR absorption bands. The interactions variability of the two independent cations and ten chloride atoms is analyzed via Hirshfeld surface analysis. [ABSTRACT FROM AUTHOR]

A novel organic–inorganic hybrid material, C 6 H 15 N 2 CdCl 3 .H 2 O, was synthesized, and its structure was determined at room temperature in the monoclinic space group P2 1 / n with the following parameters: a = 10.3829 (17), b = 7.7459 (12), c = 14.905 (2) Å, β = 98.801 (15), and Z = 4. Its crystal structure is characterized by one-dimensional polymeric chains of edge-sharing CdCl 5 N distorted octahedra. These chains are linked to the water molecules via O H … Cl hydrogen bonds to form layers parallel to the ( b , a + c ) plane. The crystal structure was stabilized by an extensive network of N H … Cl, O H … Cl and N H … O hydrogen bonds. The differential scanning calorimetry (DSC) reveals that the title compound is stable until 101.6 °C. The optimized geometry parameters, normal mode frequencies, and corresponding vibrational assignments of the present compound were theoretically examined by DFT/B3LYP method with the Lanl2dz basis set. The FT-IR spectrum of the polycrystalline sample was examined and compared to the calculated spectrum. The calculated results showed that the optimized geometry could well reproduce the crystal structure and that the theoretical vibrational frequency values were in good agreement with their experimental counterparts. [ABSTRACT FROM AUTHOR]

The chemical preparation, crystal structure, Hirshfeld surface analysis and spectroscopic characterization of the novel cadmium (II) 4-hydroxy-1-methylpiperidine complex, Cd 4 Cl 10 (C 6 H 14 NO) 2 ·2H 2 O, have been reported. The atomic arrangement can be described as built up by an anionic framework, formed by edge sharing CdCl 6 and CdCl 5 O octahedral linear chains spreading along the a -axis. These chains are interconnected by water molecules via O–H⋯Cl and O–H⋯O hydrogen bonds to form layers parallel to (011) plane. The organic cations are inserted between layers through C–H⋯Cl hydrogen bonds. Investigation of intermolecular interactions and crystal packing via Hirshfeld surface analysis reveals that the H C ⋯Cl and H C ⋯H C intermolecular interactions are the most abundant contacts of the organic cation in the crystal packing. The statistical analysis of crystal contacts reveals the driving forces in the packing formation. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks and of the IR bands. [ABSTRACT FROM AUTHOR]

The chemical preparation, crystal structure and spectroscopic characterization of the novel noncentrosymmetric (S)nicotiniumtrichloridozincate monohydrate complex are reported. The atomic arrangement can be described as built up by chains of ZnNCl 3 tetrahedra and water molecules, interconnected via O–H…Cl hydrogen bonds. The organic entities are inserted between these chains through C–H…Cl and N–H…Cl hydrogen bonds. The 3D Hirshfeld surfaces and the associated 2D fingerprint plots were investigated for intermolecular interactions. The 13 C and 15 N CP-MAS NMR spectra are in agreement with the X-ray structure. The vibrational absorption bands were identified by infrared spectroscopy. DFT calculations allowed the attribution of the NMR peaks. [ABSTRACT FROM AUTHOR]

The inorganic–organic hybrid compound (C 9 N 4 H 28 )Cd 7 (H 2 O) 2 Cl 18 · n H 2 O( n = 5.89) features an unusual cadmium chloride structure. The title complex adopts a layered structure consisting of double-chains and tetramers of [Cd ϕ 6 ] ( ϕ = Cl, O) octahedra. Crystallization water molecules and [C 9 H 28 N 4 ] 4+ tetracations are located in interstices of the successive corrugated layers. This compound has also been investigated by FT-IR and solid-state 13 C, 15 N CP-MAS and 2D 13 C-H NMR spectroscopies. [ABSTRACT FROM AUTHOR]

The synthesis and the structure of (C 10 H 15 N 2 ) 4 (Li) 2 (P 6 O 18 )(H 2 O) 6 are described. This compound crystallizes in the triclinic system, with the centric space group P-1 and the following unit cell parameters: a  = 9.7762(6), b  = 10.2502(8), c  = 15.2173(11) Å, α  = 92.588(4), β  = 98.855(4), γ  = 115.724(4)°, Z  = 2 and V  = 1346.62(17) Å 3 . The crystal structure has been solved and refined to R  = 0.0452 and Rw  = 0.1121. [Li 2 (P 6 O 18 )(H 2 O)] 4- entities are associated by strong O H⋯O hydrogen bonds to form inorganic layers lying in the (a, b) plane. These layers are interconnected with the organic entities via N H⋯O and C H⋯O hydrogen bonds. In this atomic arrangement, H bonds between the different species play an important role in the three-dimensional network. The contacts enrichment ratios derived from the Hirshfeld surface analysis show that the crystal packing is stabilized by ionic bridges Li + … O, strong N/O H⋯O hydrogen bonds but also hydrophobic interactions between the two independant 1-phenylpiperazine-1,4-dium ligands. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of the new compound were computed. The title compound was further characterized by FT-IR and NMR spectroscopies. The crystal symmetry was confirmed by 31 P and 7 Li MAS NMR and the vibrational absorption bands were identified by infrared spectroscopy. The new compound was also characterized by thermal analysis to determine the thermal behavior. [ABSTRACT FROM AUTHOR]

Two new organic-inorganic hybrid materials, 4-methoxybenzylammonium nitrate, (C 8 H 12 NO)·[NO 3 ] (I) , and 2-(1-piperazinyl)pyrimidinium bis(perchlorate), (C 8 H 14 N 4 )·[ClO 4 ] 2 (II) , have been synthesized by an acid/base reaction at room temperature, their structures were determined by single crystal X-ray diffraction. Compound (I) crystallizes in the orthorhombic system and Pnma space group with a  = 15.7908 (7), b  = 6.8032 (3), c  = 8.7091 (4) Å, V  = 935.60 (7) Å 3 with Z  = 4. Full-matrix least-squares refinement converged at R  = 0.038 and w R ( F 2 ) = 0.115. Compound (II) belongs to the monoclinic system, space group P 2 1 / c with the following parameters: a  = 10.798(2), b  = 7.330(1), c  = 21.186(2) Å, β  = 120.641 (4)°, V  = 1442.7 (3) Å 3 and Z  = 4. The structure was refined to R  = 0.044, w R ( F 2 ) = 0.132. In the structures of ( I ) and ( II ), the anionic and cationic entities are interconnected by hydrogen bonding contacts forming three-dimensional networks. Intermolecular interactions were investigated by Hirshfeld surfaces and the contacts of the four different chloride atoms in (II) were compared. The Molecular Electrostatic Potential (MEP) maps and the HOMO and LUMO energy gaps of both compounds were computed. The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13 C, 35 Cl and 15 N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. [ABSTRACT FROM AUTHOR]

The reaction of perchloric acid with 1-(2-aminoethyl)piperazine or 5,6-dimethyl-benzimidazole results in the formation of 1-(2-amonioethyl)piperazine-1,4-dium triperchlorate hydrate (C 6 H 18 N 3 )·(ClO 4 ) 3 ·H 2 O (I) or 5,6-dimethyl-benzylimidazolium perchlorate (C 9 H 11 N 2 )·ClO 4 (II) . Both compounds were fully structurally characterized including single crystal X-ray diffraction analysis. Compound (I) crystallizes in the centrosymmetric triclinic space group P 1 ¯ with the lattice parameters a = 7.455 (2), b = 10.462 (2), c = 10.824 (2) Å, α = 80.832 (2), β = 88.243 (2), γ = 88.160 (2) °, Z = 2 and V = 832.77 (3) Å 3 . Compound (II) has been found to belong to the P 2 1 /c space group of the monoclinic system, with a  = 7.590 (3), b  = 9.266 (3), c  = 16.503 (6) Å, β = 107.38 (2) °, V = 1107.69 (7) Å 3 and Z = 4. The structures of (I) and (II) consist of slightly distorted [ClO 4 ] - tetrahedra anions and 1-(2-amonioethyl)piperazine-1,4-dium trication (I) or 5,6-dimethyl-benzylimidazolium cations (II) and additionally a lattice water in (I) . The crystal structures of ( I) and ( II) exhibit complex three-dimensional networks of H-bonds connecting all their components. In the atomic arrangement of (I) , the ClO 4 − anions form corrugated chains, while in (II) the atomic arrangement exhibits wide pseudo-hexagonal channels of ClO 4 tetrahedra including the organic entities. The lattice water serves as a link between pairs of cations and pairs of anions via several O H⋯O and N-H⋯O interactions in compound (I) . The vibrational absorption bands were identified by infrared spectroscopy. These compounds were also investigated by solid-state 13 C, 35 Cl and 15 N NMR spectroscopy. DFT calculations allowed the attribution of the IR and NMR bands. Intermolecular interactions were investigated by Hirshfeld surfaces. Electronic properties such as HOMO and LUMO energies were derived. [ABSTRACT FROM AUTHOR]

(C 6 H 7 FN) 4 (Li) 2 (P 6 O 18 ) (H 2 O) 6 (I) , a new organic cyclohexaphosphate, has been synthesized and grown at room temperature by an acid/base reaction between H 6 P 6 O 18 and 2-fluoroaniline as an organic template. The crystal structure of (I) was solved by single crystal X-ray diffraction analysis and it was found that the material belongs to triclinic system with space group P-1 and refined R -factor of 0.0520. Adjacent P 6 O 18 rings are connected via corner-sharing by LiO 4 tetrahedra, generating anionic [Li 2 P 6 O 18 ·H 2 O] 4- layers parallel to the ( a , b ) plane. The 2-fluoro-anilinium cations are inserted in the interlayer space and interact with the inorganic framework through N H⋯O and O H⋯O hydrogen-bonding interactions. Additional stabilization is provided by strong N H⋯F and weak C H⋯O hydrogen bonds. Hirshfeld surface analysis reveals the nature of intermolecular contacts of the title compound and their enrichment ratio reveals if they are over-represented. The crystal packing is a combination of strong electrostatic attractive interactions and of weaker hydrophobic contacts. The title compound was further characterized by FT-IR and NMR spectroscopies. Crystal symmetry is confirmed by 31 P magic angle spinning NMR and the vibrational absorption bands were identified by infrared spectroscopy. Electrical conductivity was studied using impedance spectroscopy and results showed that the conductivity at 150 °C was equal to 4.93 × 10 −4  S cm −1 . It is therefore concluded that (C 6 H 7 FN) 4 (Li) 2 (P 6 O 18 ) (H 2 O) 6 can be further used in lithium batteries. [ABSTRACT FROM AUTHOR]

• New dihydropyrimidines. • Conformational analysis. • Hirshfeld surface analysis. We report herein the synthesis of new derivatives of dihydropyrimidine on the basis of 2,4,6-trimetoxybenzaldehyde , which was further regioselectively oxidized in the presence of cerium ammonium nitrate (CAN) with the formation of 5-acetyl-6-methyl-4-(2,4,6-trimethoxyphenyl)pyrimidin-2(1H)-one. The structures of both novel compounds were investigated by NMR, mass spectroscopy methods. The structure of the dihydropyrimidine compound 4 was also investigated by X-ray single crystal diffraction method. In order to understand the molecular interactions in its crystal packing, the Hirshfeld surface and contacts enrichment analyses were performed. Biological activities of the synthesized compounds were studied against gram-negative A. baumanii, E. coli, P. aeruginosa and K. pneumoniae and gram-positive S. aureus bacteria. [Display omitted] [ABSTRACT FROM AUTHOR]

The synthesis and investigation of a new biologically active derivative of dihydropyrimidine are reported. The structure of the synthesized compound was investigated by X-ray single crystal diffraction method. In order to understand the molecular interactions, the Hirshfeld surface and contacts enrichment analyses were performed. The crystal packing is mainly stabilized by strong N–H⋯O hydrogen bonds and aromatic cycle stacking. Among the different types of oxygen atoms, the most electronegative had the highest propensity to form H-bonds. Biological activity of the synthesized compound was studied against E.coli , P. aeruginosa and S. aureus bacteria. Image 1 • New Biginelli compound. • Conformational analysis. • Hirshfeld surface analysis. [ABSTRACT FROM AUTHOR]